WO2021027264A1 - 一种精确表征晶体三维取向和晶体学取向的方法 - Google Patents

一种精确表征晶体三维取向和晶体学取向的方法 Download PDF

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WO2021027264A1
WO2021027264A1 PCT/CN2020/073163 CN2020073163W WO2021027264A1 WO 2021027264 A1 WO2021027264 A1 WO 2021027264A1 CN 2020073163 W CN2020073163 W CN 2020073163W WO 2021027264 A1 WO2021027264 A1 WO 2021027264A1
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dimensional
orientation
ebsd
characteristic
crystallographic
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陈国清
王雅琨
付雪松
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大连理工大学
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/20058—Measuring diffraction of electrons, e.g. low energy electron diffraction [LEED] method or reflection high energy electron diffraction [RHEED] method
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
    • G01N23/04—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material
    • G01N23/046—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material using tomography, e.g. computed tomography [CT]
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/203—Measuring back scattering
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/2202—Preparing specimens therefor
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
    • G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/05—Investigating materials by wave or particle radiation by diffraction, scatter or reflection
    • G01N2223/053—Investigating materials by wave or particle radiation by diffraction, scatter or reflection back scatter
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/40—Imaging
    • G01N2223/418—Imaging electron microscope
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/60—Specific applications or type of materials
    • G01N2223/602—Specific applications or type of materials crystal growth
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/60—Specific applications or type of materials
    • G01N2223/606—Specific applications or type of materials texture

Definitions

  • the invention relates to the technical field of material analysis, in particular to a method for accurately characterizing three-dimensional crystal orientation and crystallographic orientation.
  • the first method is to make three-dimensional observations of materials through Computed Tomography (CT) technology.
  • Commonly used light sources include synchrotron X-ray sources and neutron-ray sources.
  • Chinese patent application CN201610118509.5 discloses a real-time X-ray stereo imaging system and imaging method based on synchrotron radiation. The method reconstructs the sample by two-dimensional projections in different directions, and combines the absorption contrast or phase contrast imaging technology to realize the three-dimensional accurate reconstruction of the sample structure.
  • the main problem of the method is that the requirements for the light source are high, the operation is complicated, and the three-dimensional orientation information of the crystal structure in the sample cannot be obtained at the same time.
  • the second method is to obtain the two-dimensional cross-sectional structure of each layer by tomography and observe the morphology, and then obtain the spatial structure morphology after three-dimensional reconstruction.
  • Chinese patent application CN201380024943.1 discloses an observation and photographing device, which is mainly based on a microscope with a photographing section that can photograph a magnified sample. The sample can be mechanically ground and imaged using a light microscope. The main problem with this method is the heavy workload and difficulty in alignment between the layers.
  • the focused ion beam electron beam system has the ability to observe and analyze the micro-nano processing of the focused ion beam and the scanning electron beam.
  • the scanning electron beam is used to observe and find the characteristic area of interest (such as defects, interfaces, etc.) of the sample, and then the area is precisely processed by the focused ion beam.
  • the FIB/SEM dual beam system can also obtain information about the chemical composition and crystal structure of the sample.
  • Chinese patent CN201710772302.4 discloses a three-dimensional characterization method for the surface coating of galvanized sheet.
  • the three-dimensional characterization method adopts the ion beam in the FIB/SEM dual beam system to cut the galvanized sheet coating, the electron beam collects relevant data of the cut section, and analyzes the coating information in combination with a three-dimensional image analysis software.
  • This method has the advantages of high accuracy and can perform orientation analysis at the same time. Therefore, the FIB/SEM dual-beam system plays an important role in material failure analysis, nano-material structure characterization and performance analysis, and nano-device development.
  • the present invention is an in-depth development and efficient use of FIB technology.
  • step 1) The series of the two-dimensional tissue morphologies obtained in step 1) are synthesized by three-dimensional image analysis software to obtain the three-dimensional morphology;
  • the two-dimensional structure morphology can be obtained through FIB/SEM double-beam system observation, or through optical microscope observation after mechanical grinding and polishing.
  • the method for obtaining the EBSD pattern is specifically obtained by analyzing EBSD data of at least one plane in the area, and the EBSD data is collected based on an EBSD probe.
  • the feature topography can determine the three-dimensional orientation of the feature surface through the slicing function in the three-dimensional image analysis software; for feature lines or rods, by extracting the normal direction of the two surfaces passing through the line or rod, Cross-multiply it to obtain the three-dimensional orientation of the characteristic line or rod.
  • the present invention extracts the three-dimensional orientation of the characteristic morphology of the reconstructed sample, obtains the spatial crystallographic orientation through coordinate conversion, and can accurately analyze the orientation and crystallographic orientation of the characteristic structure of the eutectic ceramic material at the same time, especially for
  • the characteristic structure of micron size has strong applicability; at the same time, it is also suitable for the microstructure analysis of various materials such as pure metals, alloys or metal matrix composite materials, inorganic non-metallic materials, etc., and it has the ability to study the crystal growth orientation and growth behavior of materials. important meaning.
  • the characteristic structure is characterized by combining the SEM image and the EBSD image, and the direction and the shape of the characteristic structure have a higher resolution than the simple 3D-EBSD.
  • the present invention can be widely promoted in the field of material analysis technology.
  • FIG. 1 is a flowchart of the operation steps of the present invention.
  • Figure 2 is a SEM picture of the region of interest in the Al 2 O 3 /ZrO 2 eutectic ceramic in Example 1 of the present invention.
  • Fig. 3 is a three-dimensional image of Al 2 O 3 /ZrO 2 eutectic ceramic after three-dimensional reconstruction in Example 1 of the present invention.
  • Figure 4 is a single slice diagram in Example 1 of the present invention.
  • Figure 5 is a reverse pole diagram of a single slice EBSD in Example 1 of the present invention.
  • the present invention provides a method for accurately characterizing three-dimensional crystal orientation and crystallographic orientation, including the following steps:
  • Pre-treating the crystal to be analyzed that is, performing work such as pre-grinding and polishing according to the measurement requirements of different crystals, placing it in the experimental area, and obtaining the crystal material through FIB/SEM dual-beam system or through optical microscope observation The two-dimensional structure morphology of a series of cross-sections in the area to be measured;
  • the EBSD pattern in the area to be tested is obtained through the EBSD data system;
  • the EBSD data system includes the EBSD probe, the control system and the corresponding processing software.
  • the probe transmits the collected EBSD pattern to the computer software for calibration, which is obtained through the channel5 software
  • the diffraction pattern corresponds to the vector in the macroscopic coordinate system to construct the EBSD crystallographic coordinate system;
  • the series of the two-dimensional tissue morphology obtained in the step 1) is synthesized by three-dimensional image analysis software to obtain the three-dimensional morphology.
  • the three-dimensional image analysis software of this embodiment adopts Avizo software. Image processing of SEM pictures, then threshold segmentation, binarization of the overall data, and automatic generation of the coordinate system of the three-dimensional topography through Avizo software;
  • step 4 Establish a conversion relationship between the crystallographic coordinate system obtained in step 2) and the coordinate system where the three-dimensional topography obtained in step 3) is located.
  • the conversion is performed manually according to the different planes of the EBSD collected.
  • the Al 2 O 3 /ZrO 2 eutectic ceramic to be analyzed is pre-ground, polished, and carbon sprayed.
  • X, Y, and Z are the bases of the three-dimensional image constructed by the SEM image. Arrow.
  • the orientation information obtained by 3D-EBSD shows that the Al 2 O 3 ceramics in this area are single crystals, and the orientations in different slice photos are consistent. Therefore, in this embodiment, the crystallographic orientation of the sample is obtained with the EBSD image of the first slice.
  • the IPF of the first slice is shown in Figure 5. Since the 70-degree correction was not performed when the EBSD image was collected, it needs to be elongated in the vertical direction, and the elongated length is 2.94 times the original length.
  • the RD, TD, and ND directions of the collected EBSD data correspond to the x, y, and z basis vector directions in the EBSD image, respectively, and the x, y, and z basis vectors obtained after normalization.
  • the structure of the ZrO 2 ceramic in this embodiment is mainly a rod-like structure, and has a surface composed of rods. Therefore, in this embodiment, a rod and a side are taken as an example to extract the characteristic structure.
  • the central axis of the rod is mainly extracted, and when extracting the feature structure of the surface, the normal orientation of the surface is extracted.
  • Use Avizo's Slice command to obtain the normals of the two faces passing through a rod, and cross-multiply the normals of the two faces to obtain the centerline direction of the rod.
  • Use Avizo's Slice command to obtain the surface normal of the characteristic surface.
  • the surface normal direction of the surface is the surface normal direction of the characteristic surface.
  • the RD, TD, and ND directions of the collected EBSD data correspond to the x, y, and z basis vector directions in the EBSD image, respectively, and the x, y, and z basis vectors obtained after normalization.
  • Extract the characteristic structure of the Si crystal grains in this embodiment The normal orientation of the surface is extracted when the surface feature structure is extracted.
  • Use Avizo's Slice command to obtain the normals of the two faces passing through a rod, and cross-multiply the normals of the two faces to obtain the centerline direction of the rod.
  • Use Avizo's Slice command to obtain the surface normal of the characteristic surface.
  • the surface normal direction of the surface is the surface normal direction of the characteristic surface.
  • the orientation information obtained by 3D-EBSD determine the orientation of the substrate in different areas. Since the 70-degree correction was not performed when the EBSD image was collected, it needs to be elongated in the vertical direction, and the elongated length is 2.94 times the original length.
  • the RD, TD, and ND directions of the collected EBSD data correspond to the x, y, and z basis vector directions in the EBSD image, respectively, and the x, y, and z basis vectors obtained after normalization.
  • the normal orientation of the surface is extracted when the surface feature structure is extracted.
  • Use Avizo's Slice command to obtain the normals of the two faces passing through a rod, and cross-multiply the normals of the two faces to obtain the centerline direction of the rod.
  • Use Avizo's Slice command to obtain the surface normal of the characteristic surface.
  • the surface normal direction of the surface is the surface normal direction of the characteristic surface.
  • the 718 nickel-based alloy to be analyzed is pre-ground and polished.
  • the RD, TD, and ND directions of the collected EBSD data correspond to the x, y, and z basis vector directions in the EBSD image, respectively, and the x, y, and z basis vectors obtained after normalization.
  • the normal orientation of the surface is extracted when the surface feature structure is extracted.
  • Use Avizo's Slice command to obtain the normals of the two faces passing through a rod, and cross-multiply the normals of the two faces to obtain the centerline direction of the rod.
  • Use Avizo's Slice command to obtain the surface normal of the characteristic surface.
  • the surface normal direction of the surface is the surface normal direction of the characteristic surface.

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Abstract

一种精确表征晶体三维取向和晶体学取向的方法，包括如下步骤：获取晶体材料待测区域内的二维组织形貌和EBSD花样；将其通过三维图像分析软件进行三维图像合成，获取三维形貌；提取特征形貌在三维形貌所在坐标系中的三维取向；通过三维取向转换到EBSD获得的晶体学坐标系中，获得特征形貌的晶体学取向。该方法同时解析各种材料特征组织结构的取向和晶体学取向，对材料晶体生长取向和生长行为研究具有重要意义。

Description

一种精确表征晶体三维取向和晶体学取向的方法 技术领域
本发明涉及材料分析技术领域，尤其涉及一种精确表征晶体三维取向和晶体学取向的方法。
背景技术
为获取材料在三维空间的显微组织结构，目前常用方法有两种。
第一种方法是通过电子计算机断层扫描技术(Computed Tomography,CT)对材料进行三维观测。常用的光源有同步辐射X射线源、中子射线源等。中国专利申请CN201610118509.5公开了一种基于同步辐射的实时X射线立体成像系统及成像方法。所述方法由样品不同方向二维投影进行重构，结合吸收衬度或相位衬度成像技术实现样品结构的三维精确重构。所述方法的主要问题是对光源的要求很高，操作复杂，无法同时获取样品中晶体结构的三维取向信息。
第二种方法是通过层析法获得每层二维截面组织并进行形貌观察，然后进行三维重构后获得空间组织形貌。中国专利申请CN201380024943.1公开了一种观察拍摄装置，所述装置主要基于一个可对放大试样进行拍摄的带有拍摄部的显微镜。所述样品可进行机械研磨，并利用光镜进行成像。此方法存在的主要问题是工作量大、层片之间的对齐困难。
聚焦离子束电子束系统具有聚焦离子束的微纳米加工与扫描电子束的观察分析能力。在FIB/SEM双束系统中，利用扫描电子束观察和寻找样品感兴趣特征区(如缺陷、界面等)，然后通过聚焦离子束对该区域进行精确加工。利用FIB/SEM双束系统还可以获取有关样品化学组分和晶体结构等方面的信息。中国专利CN201710772302.4公开了一种镀锌板表面镀层的三维表征方法。所述三维表征方法是采用FIB/SEM双束系统中离子束对镀锌板镀层进行切割，电子束采集切割截面的相关数据，并结合三维图像分析软件分析镀层的信息。 该方法具有准确度高，可以同时进行取向分析的优点。因此FIB/SEM双束系统在材料失效分析、纳米材料结构表征与性能分析以及纳米器件研制等方面发挥着重要作用，本发明是对FIB技术的深层次开发和高效利用。
发明内容
根据上述提出的技术问题，而提供一种精确表征晶体三维取向和晶体学取向的方法。本发明采用的技术手段如下：
一种精确表征晶体三维取向和晶体学取向的方法，包括如下步骤：
1)获取所述晶体材料待测区域内的一系列截面的二维组织形貌；
2)获取待测区域内EBSD花样；
3)将所述步骤1)获得的系列所述二维组织形貌通过三维图像分析软件进行三维图像合成，获取三维形貌；
4)在EBSD获得的晶体学坐标系与所述三维形貌所在坐标系之间建立转换关系；
5)在所述步骤3)中合成的所述三维形貌中提取特征形貌在三维形貌所在坐标系中的三维取向；
6)将所述步骤5)的特征形貌的三维取向转换到EBSD获得的晶体学坐标系中，获得所述特征形貌的晶体学取向。
进一步地，所述二维组织形貌的获取具体通过FIB/SEM双束系统观察获得，或者经机械磨抛后通过光学显微镜观察获得。
进一步地，所述EBSD花样的获取方法具体通过分析区域内至少一个平面的EBSD数据获得，所述EBSD数据基于EBSD探头进行采集。
进一步地，所述特征形貌能够通过在三维图像分析软件中的切片功能确定特征面的三维取向；对于特征线或棒，通过提取穿过所述线或棒的两个面的法线方向，对其进行叉乘，获得所述特征线或棒的三维取向。
本发明对重构后样品的特征形貌的三维取向进行提取，通过坐标转换，获得空间上的晶体学取向，可以精确地同时解析共晶陶瓷材料特征组织结构 的取向和晶体学取向，尤其对于微米尺寸的特征结构具有极强的适用性；同时也适用于纯金属、合金或金属基复合材料、无机非金属材料等各种材料的显微组织分析，对材料晶体生长取向和生长行为研究具有重要意义。本发明通过结合SEM图像和EBSD图像进行特征结构表征，对于特征结构的方向和形貌比单纯做3D-EBSD的分辨率更高。
基于上述理由本发明可在材料分析技术领域广泛推广。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图做以简单地介绍，显而易见地，下面描述中的附图是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动性的前提下，还可以根据这些附图获得其他的附图。
图1为本发明操作步骤流程图。
图2为本发明实施例1中Al 2O 3/ZrO 2共晶陶瓷中感兴趣区域的SEM图片。
图3为本发明实施例1中Al 2O 3/ZrO 2共晶陶瓷三维重构后三维图像。
图4为本发明实施例1中单张切片图。
图5为本发明实施例1中单张切片EBSD的反极图。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚，下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
本发明提供了一种精确表征晶体三维取向和晶体学取向的方法，包括如下步骤：
1)对待分析的晶体进行预处理，即根据不同晶体的测量要求进行诸如预 磨、抛光等工作，将其置于实验区域，通过FIB/SEM双束系统或者通过光学显微镜观察获取所述晶体材料待测区域内的一系列截面的二维组织形貌；
2)同时，通过EBSD数据系统获取待测区域内EBSD花样；EBSD数据系统包括EBSD探头和控制系统以及相应的处理软件，探头将采集到的EBSD花样传送到计算机软件进行标定，通过channel5软件获得的衍射花样对应到宏观坐标系下的矢量，构筑EBSD的晶体学坐标系；
3)将所述步骤1)获得的系列所述二维组织形貌通过三维图像分析软件进行三维图像合成，获取三维形貌，本实施例的三维图像分析软件采用Avizo软件，对导入Avizo软件的SEM图片进行图像处理，之后进行阈值分割，对整体数据进行二值化处理，通过Avizo软件自动生成三维形貌所在坐标系；
4)对步骤2)获得的晶体学坐标系与和步骤3)获得的三维形貌所在坐标系之间建立转换关系，具体根据采集EBSD的平面不同进行人为转换，本实施例中，Avizo中定义的X、Y、Z基矢方向和EBSD图像中的x、y、z基矢方向的关系为：X＝x；Y＝-1*y；Z＝z；
5)在所述步骤3)中合成的所述三维形貌中提取特征形貌在三维形貌所在坐标系中的三维取向；根据不同晶体的棒结构或者面结构进行不同的特征形貌提取，提取棒的特征形貌时主要提取棒的中轴线，提取面特征结构时提取面的法线取向。通过Avizo的Slice命令获取通过一个棒的两个面法线，并对两个面的面法线叉乘获取棒的中心线方向；通过Avizo的Slice命令获取特征面的面法线，该面的面法线方向即为特征面的面法线方向。
6)将所述步骤5)的特征形貌的三维取向转换到EBSD获得的晶体学坐标系中，获得所述特征形貌的晶体学取向。
实施例一：
1.首先对待分析的Al 2O 3/ZrO 2共晶陶瓷进行预磨、抛光，并进行喷碳处理。
2.采用FIB(聚焦离子束)/SEM(扫描电子显微镜)双束系统(Helios G4UX,FEI)结合EBSD(电子背散射衍射)探头(Oxford)进行三维重构和三维 EBSD表征。通过背散射电子图像观察合适的表征区域。本次进行三维重构区域如附图2所示。进行三维重构区域为20*10*10μm 3，其中深度方向为10μm。选定区域后对周围区域进行挖坑，将要进行三维重构的区域焊接到铜环上。然后设定程序进行离子束切割，通过SEM成像使用的电子束和EBSD探头采集数据。每隔100nm采集一张SEM图片，每隔200nm采集一张EBSD图片。
3.将采集的SEM图片导入Avizo中，切片厚度设为100nm。然后按照DualBeam 3D Wizard中的步骤进行处理。本实施例中采集的SEM图片没有畸变，所以无需进行矫正。分别按顺序进行以下步骤：图片剪切、将存在问题的切片删除、对齐处理、再剪切图片最终确定感兴趣区域、滤波、降噪、亮度矫正(本实施例跳过降噪、亮度矫正两步骤)。完成后进行阈值分割，对整体数据进行二值化处理，将ZrO 2相对应灰度值范围统一定义为1，Al 2O 3相对应灰度值范围统一定义为0。将选中的ZrO 2相区域进行三维显示的组织形貌如附图3所示。在Avizo中定义X、Y、Z三个基矢方向(左手定则)，在切片上观察如附图4所示，归一化后X、Y、Z分别为SEM图像构建的三维图像的基矢。
4.通过3D-EBSD获得的取向信息可知，该区域Al 2O 3陶瓷为单晶体，不同切片照片中取向均一致。所以本实施例以第一张切片的EBSD图片获取样品的晶体学取向。第一张切片的反极图(IPF)如附图5所示。由于采集EBSD图像时未进行70度矫正，需要在竖直方向上进行拉长，拉长后长度为2.94倍原始长度。采集的EBSD数据的RD、TD、ND方向分别对应EBSD图像中的x、y、z基矢方向，进行归一化后获得的x、y、z基矢。
通过实验中几何关系可知Avizo中定义的X、Y、Z基矢方向和EBSD图像中的x、y、z基矢方向的关系为：
X＝x；Y＝-1*y；Z＝z。
5.本实施例中的ZrO 2陶瓷的组织形貌以棒状结构为主，且有棒组成的面。所以本实施例以一棒和一面为例进行提取特征结构。提取棒的特征形貌时主要提取棒的中轴线，提取面特征结构时提取面的法线取向。通过Avizo的Slice命令获取通过一个棒的两个面法线，并对两个面的面法线叉乘获取棒的中心线方向。通过Avizo的Slice命令获取特征面的面法线，该面的面法线方向即 为特征面的面法线方向。通过上述的X、Y、Z和x、y、z的相互转换可获得特征取向在晶体学坐标系中的取向。
实施例二：
1.首先对待分析的铸造多晶硅进行预磨、抛光。
2.采用FIB/SEM双束系统(Helios G4 UX,FEI)结合EBSD探头(Oxford)进行三维重构和三维EBSD表征。通过二次电子图像观察合适的表征区域。进行三维重构区域为20*10*10μm 3，其中深度方向为10μm。选定区域后对周围区域进行挖坑，将要进行三维重构的区域焊接到铜环上。然后设定程序进行离子束切割，电子束和EBSD探头采集数据。每隔100nm采集一张SEM图片，每隔200nm采集一张EBSD图片。
3.将采集的SEM图片导入Avizo中，切片厚度设为100nm。然后按照DualBeam 3D Wizard中的步骤进行处理。本工作中采集的SEM图片没有畸变，所以无需进行矫正。分别按顺序进行以下步骤：图片剪切、将存在问题的切片删除、对齐处理、再剪切图片最终确定感兴趣区域、滤波、降噪、亮度矫正(本工作跳过降噪、亮度矫正两步骤)。完成后进行阈值分割，对整体数据进行二值化处理，将一侧Si晶粒对应灰度值范围统一定义为1，另一侧Si晶粒对应灰度值范围统一定义为0。将选中的一侧Si晶粒区域进行三维显示。在Avizo中定义X、Y、Z三个基矢方向(左手定则)，归一化后X、Y、Z分别为SEM图像构建的三维图像的基矢。
4.通过3D-EBSD获得的取向信息，确定不同区域的Si取向。由于采集EBSD图像时未进行70度矫正，需要在竖直方向上进行拉长，拉长后长度为2.94倍原始长度。采集的EBSD数据的RD、TD、ND方向分别对应EBSD图像中的x、y、z基矢方向，进行归一化后获得的x、y、z基矢。
通过实验中几何关系可知Avizo中定义的X、Y、Z基矢方向和EBSD图像中的x、y、z基矢方向的关系为：
X＝x；Y＝-1*y；Z＝z。
5.提取本实施例中的Si晶粒的特征结构。提取面特征结构时提取面的法线取向。通过Avizo的Slice命令获取通过一个棒的两个面法线，并对两个面的面法线叉乘获取棒的中心线方向。通过Avizo的Slice命令获取特征面的面 法线，该面的面法线方向即为特征面的面法线方向。通过X、Y、Z和x、y、z的相互转换可获得特征取向在晶体学坐标系中的取向。
实施例三：
1.首先对待分析的Al-Si共晶合金进行预磨、抛光。
2.采用FIB/SEM双束系统(Helios G4 UX,FEI)结合EBSD探头(Oxford)进行三维重构和三维EBSD表征。通过背散射电子图像观察合适的表征区域。进行三维重构区域为20*10*10μm 3，其中深度方向为10μm。选定区域后对周围区域进行挖坑，将要进行三维重构的区域焊接到铜环上。然后设定程序进行离子束切割，电子束和EBSD探头采集数据。每隔100nm采集一张SEM图片，每隔200nm采集一张EBSD图片。
3.将采集的SEM图片导入Avizo中，切片厚度设为100nm。然后按照DualBeam 3D Wizard中的步骤进行处理。本工作中采集的SEM图片没有畸变，所以无需进行矫正。分别按顺序进行以下步骤：图片剪切、将存在问题的切片删除、对齐处理、再剪切图片最终确定感兴趣区域、滤波、降噪、亮度矫正(本工作跳过降噪、亮度矫正两步骤)。完成后进行阈值分割，对整体数据进行二值化处理，将初生Si相对应灰度值范围统一定义为1，基体相对应灰度值范围统一定义为0。将选中的初生Si相区域进行三维显示。在Avizo中定义X、Y、Z三个基矢方向(左手定则)，归一化后X、Y、Z分别为SEM图像构建的三维图像的基矢。
4.通过3D-EBSD获得的取向信息，确定不同区域的基体取向。由于采集EBSD图像时未进行70度矫正，需要在竖直方向上进行拉长，拉长后长度为2.94倍原始长度。采集的EBSD数据的RD、TD、ND方向分别对应EBSD图像中的x、y、z基矢方向，进行归一化后获得的x、y、z基矢。
通过实验中几何关系可知Avizo中定义的X、Y、Z基矢方向和EBSD图像中的x、y、z基矢方向的关系为：
X＝x；Y＝-1*y；Z＝z。
5.提取本实施例中的单晶Si相的特征结构。提取面特征结构时提取面的法线取向。通过Avizo的Slice命令获取通过一个棒的两个面法线，并对两个面的面法线叉乘获取棒的中心线方向。通过Avizo的Slice命令获取特征面的 面法线，该面的面法线方向即为特征面的面法线方向。通过X、Y、Z和x、y、z的相互转换可获得特征取向在晶体学坐标系中的取向。
实施例四：
1.首先对待分析的718镍基合金进行预磨、抛光。
2.采用FIB/SEM双束系统(Helios G4 UX,FEI)结合EBSD探头(Oxford)进行三维重构和三维EBSD表征。通过背散射电子图像观察合适的表征区域。进行三维重构区域为20*10*10μm 3，其中深度方向为10μm。选定区域后对周围区域进行挖坑，将要进行三维重构的区域焊接到铜环上。然后设定程序进行离子束切割，电子束和EBSD探头采集数据。每隔100nm采集一张SEM图片，每隔200nm采集一张EBSD图片。
3.将采集的SEM图片导入Avizo中，切片厚度设为100nm。然后按照DualBeam 3D Wizard中的步骤进行处理。本工作中采集的SEM图片没有畸变，所以无需进行矫正。分别按顺序进行以下步骤：图片剪切、将存在问题的切片删除、对齐处理、再剪切图片最终确定感兴趣区域、滤波、降噪、亮度矫正(本工作跳过降噪、亮度矫正两步骤)。完成后进行阈值分割，对整体数据进行二值化处理，将Laves相对应灰度值范围统一定义为1，基体相对应灰度值范围统一定义为0。将选中的Laves相区域进行三维显示。在Avizo中定义X、Y、Z三个基矢方向(左手定则)，归一化后X、Y、Z分别为SEM图像构建的三维图像的基矢。
4.通过3D-EBSD获得的取向信息，确定基体取向。由于采集EBSD图像时未进行70度矫正，需要在竖直方向上进行拉长，拉长后长度为2.94倍原始长度。采集的EBSD数据的RD、TD、ND方向分别对应EBSD图像中的x、y、z基矢方向，进行归一化后获得的x、y、z基矢。
通过实验中几何关系可知Avizo中定义的X、Y、Z基矢方向和EBSD图像中的x、y、z基矢方向的关系为：
X＝x；Y＝-1*y；Z＝z。
5.提取本实施例中的Laves相的特征结构。提取面特征结构时提取面的法线取向。通过Avizo的Slice命令获取通过一个棒的两个面法线，并对两个面的面法线叉乘获取棒的中心线方向。通过Avizo的Slice命令获取特征面的面法线，该面的面法线方向即为特征面的面法线方向。通过X、Y、Z和x、 y、z的相互转换可获得特征取向在晶体学坐标系中的取向。
最后应说明的是：以上各实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述各实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分或者全部技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的范围。

Claims (4)

  1. 一种精确表征晶体三维取向和晶体学取向的方法，其特征在于，包括如下步骤：
    1)获取所述晶体材料待测区域内的一系列截面的二维组织形貌；
    2)获取待测区域内EBSD花样；
    3)将所述步骤1)获得的系列所述二维组织形貌通过三维图像分析软件进行三维图像合成，获取三维形貌；
    4)在EBSD获得的晶体学坐标系与所述三维形貌所在坐标系之间建立转换关系；
    5)在所述步骤3)中合成的所述三维形貌中提取特征形貌在三维形貌所在坐标系中的三维取向；
    6)将所述步骤5)的特征形貌的三维取向转换到EBSD获得的晶体学坐标系中，获得所述特征形貌的晶体学取向。
  2. 根据权利要求1所述的精确表征晶体三维取向和晶体学取向的方法，其特征在于，所述二维组织形貌的获取具体通过FIB/SEM双束系统观察获得，或者经机械磨抛后通过光学显微镜观察获得。
  3. 根据权利要求1或2所述的精确表征晶体三维取向和晶体学取向的方法，其特征在于，所述EBSD花样的获取方法具体通过分析区域内至少一个平面的EBSD数据获得，所述EBSD数据基于EBSD探头进行采集。
  4. 根据权利要求1所述的精确表征晶体三维取向和晶体学取向的方法，其特征在于，所述特征形貌能够通过在三维图像分析软件中的切片功能确定特征面的三维取向；对于特征线或棒，通过提取穿过所述线或棒的两个面的法线方向，对其进行叉乘，获得所述特征线或棒的三维取向。
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102103093A (zh) * 2009-12-22 2011-06-22 鞍钢股份有限公司 一种大尺寸晶粒取向的检测方法
CN103928363A (zh) * 2014-04-11 2014-07-16 常州天合光能有限公司 一种硅片晶向检测方法及检测装置
US20180080884A1 (en) * 2016-09-22 2018-03-22 Advanced Manufacturing LLC Macrotexture Map Visualizing Texture Heterogeneity in Polycrystalline Parts
CN108226198A (zh) * 2017-12-27 2018-06-29 北京北冶功能材料有限公司 钢铁材料裂纹形成时段的ebsd晶粒取向判定方法
CN110441342A (zh) * 2019-08-09 2019-11-12 大连理工大学 一种精确表征晶体三维取向和晶体学取向的方法

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB0117892D0 (en) * 2001-07-23 2001-09-12 Oxford Instr Analytical Ltd Method of analysing crystalline texture
DE102012202519A1 (de) * 2012-02-17 2013-08-22 Carl Zeiss Microscopy Gmbh Verfahren und Vorrichtungen zur Präparation mikroskopischer Proben mit Hilfe von gepulstem Licht
JP5874074B2 (ja) 2012-06-21 2016-03-01 国立大学法人 鹿児島大学 観察撮影装置
CN104677709A (zh) * 2015-02-12 2015-06-03 江苏省沙钢钢铁研究院有限公司 一种制备特定晶体取向关系界面hrtem样品的方法
JP6314890B2 (ja) * 2015-03-30 2018-04-25 住友金属鉱山株式会社 結晶方位の解析方法および解析装置
CN105136829B (zh) * 2015-08-03 2017-12-05 华东交通大学 确定ebsd花样中晶体倒易矢量的二维几何关系的方法
CN105021637B (zh) * 2015-08-03 2017-07-04 华东交通大学 基于ebsd花样确定晶体倒易初基胞基矢的方法
CN105739232B (zh) 2016-03-02 2018-01-16 中国科学院上海应用物理研究所 一种基于同步辐射的实时x射线立体成像系统及成像方法
EP3535098B1 (en) * 2016-11-04 2024-03-20 UES, Inc. Automated high speed metallographic system
CN107607744A (zh) 2017-08-31 2018-01-19 武汉钢铁有限公司 镀锌板表面镀层的三维表征方法
CN110095486B (zh) * 2019-05-08 2021-12-17 中国科学院金属研究所 一种快速呈现多晶材料特定晶面分布特征的方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102103093A (zh) * 2009-12-22 2011-06-22 鞍钢股份有限公司 一种大尺寸晶粒取向的检测方法
CN103928363A (zh) * 2014-04-11 2014-07-16 常州天合光能有限公司 一种硅片晶向检测方法及检测装置
US20180080884A1 (en) * 2016-09-22 2018-03-22 Advanced Manufacturing LLC Macrotexture Map Visualizing Texture Heterogeneity in Polycrystalline Parts
CN108226198A (zh) * 2017-12-27 2018-06-29 北京北冶功能材料有限公司 钢铁材料裂纹形成时段的ebsd晶粒取向判定方法
CN110441342A (zh) * 2019-08-09 2019-11-12 大连理工大学 一种精确表征晶体三维取向和晶体学取向的方法

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